CN104987731A - One-dimension nanochain-typed Fe3O4/silk protein compound and preparation method thereof - Google Patents
One-dimension nanochain-typed Fe3O4/silk protein compound and preparation method thereof Download PDFInfo
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- CN104987731A CN104987731A CN201510382554.7A CN201510382554A CN104987731A CN 104987731 A CN104987731 A CN 104987731A CN 201510382554 A CN201510382554 A CN 201510382554A CN 104987731 A CN104987731 A CN 104987731A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 102000004169 proteins and genes Human genes 0.000 title abstract description 6
- 108090000623 proteins and genes Proteins 0.000 title abstract description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract 10
- 150000001875 compounds Chemical class 0.000 title abstract 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000012460 protein solution Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002086 nanomaterial Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012456 homogeneous solution Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013456 study Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Peptides Or Proteins (AREA)
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Abstract
The invention belongs to the technical field of materials chemistry, and particularly relates to a one-dimension nanochain-typed Fe3O4/silk protein compound and a preparation method thereof. The compound comprises Fe3O4 nano particles and silk protein, wherein the silk protein is coated with the Fe3O4 nano particles to form spherical compounds; the plurality of spherical compounds are connected to form a chain under the action of a magnetic field. According to the one-dimension nanochain-typed Fe3O4/silk protein compound and the preparation method thereof, provided by the invention, the raw materials in the synthetic method are extensive in source, and the synthetic method is simple in process.
Description
Technical field
The invention belongs to material chemistry technical field, particularly relate to a kind of 1-dimention nano chain Fe
3o
4/ silk-protein mixture and preparation method thereof.
Background technology
As everyone knows, nano material, due to the characteristic of its excellence, is applied to every field, and the progress of preparation to novel material of the nano material of specific morphology and structure is significant.The nano material of one dimension self-assembly, because of many uses, can be used for each side such as nanoelectronic, photoelectron, nanomagnets and biosensing apparatus, especially attracts the eyeball of researcher.
In recent years, one-dimensional magnetic nano material receives to be paid close attention to widely, and it all has remarkable contribution at transfer transport, magnetic conversion, DNA separation and other biological medical field.One-dimensional magnetic nano material is formed in upholder or solution by ferromegnetism and superparamagnetic nanoparticle usually, and scientists is explored the influence factor that its one-dimentional structure is formed.First, block-shaped magnetic material anisotropy is very little, be easy to when crystal field exists disappear, but under nanoscale, the relatively more atom of nanocrystal surface can make its track restore on lower collaborative face, thus form larger magnetic anisotropy energy, be conducive to the formation of one-dimensional catenary structure.Secondly, the dimensional effect caused by the change of electric field structure is also important factor in order, and the electric field structure change caused when organic molecule clad nano magneticsubstance can make the ferromegnetism behavior of material change, thus causes the formation of special construction.In addition, the formation of 1-dimention nano chain may be also due to nanoparticle between electrostatic interaction and other power effect caused by.Although there have been many exploratory studys to attempt to improve the efficiency and level preparing one-dimensional magnetic nanochain, the effective ways that one-dimensional magnetic nano material is prepared in exploration exploitation have remained key issue urgently to be resolved hurrily.
Meanwhile, silk-protein has good biocompatibility, effectively can control preparation and the pattern of nano material, and successfully prepare different nano materials, but 1-dimention nano chain Fe
3o
4the synthesis of/silk-protein mixture not yet has report.
Because above-mentioned defect, the design people, actively in addition research and innovation, to founding a kind of Wei Na meter chain Fe
3o
4/ silk-protein mixture and preparation method thereof, makes it have more utility value in industry.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide a kind of 1-dimention nano chain Fe
3o
4/ silk-protein mixture and preparation method thereof, its preparation method is simple.
A kind of 1-dimention nano chain Fe that the present invention proposes
3o
4/ silk-protein mixture, comprises Fe
3o
4nanoparticle and silk-protein, described Fe
3o
4nanoparticle is coated on described silk-protein and forms globular complex, and described in several, globular complex connects into chain.
The invention allows for 1-dimention nano chain Fe
3o
4the preparation method of/silk-protein mixture, comprises the following steps:
(1) silk-protein and source of iron are dissolved in solvent, stir and disperse;
(2) solution in described step (1) is poured in reactor, bottom reactor, place one block of magnet, at 160-200 DEG C, react 1-36h;
(3), after having reacted, product is through washing, centrifugal and dry.
Further, described source of iron is FeCl
36H
2o, the mass percentage of described silk protein solution intermediate filment is 7%.
Further, described solvent is ethylene glycol, and described step (1) is first by CH
3cOONa3H
2after O and source of iron are dissolved in ethylene glycol, then add silk-protein, stir and disperse.
Further, described FeCl
36H
2o, CH
3cOONa3H
2the mass ratio of O, ethylene glycol and silk protein solution is: (1-1.5): (5-6): (55.5-77.7): (8-12).
Further, described magnet is Fe-Nd-B magnet.
By such scheme, the present invention at least has the following advantages: the present invention using silk-protein as carrier, load Fe
3o
4nanoparticle, this mixture is chain, and its preparation method is simple, uses magnet to induce Fe as externally-applied magnetic field during preparation
3o
4the magnetic domain orientation of nanoparticle is consistent, makes this mixture have stronger saturation magnetic field, and synthesis material wide material sources, and synthetic method craft is simple.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention one;
Fig. 2 is the transmission electron microscope picture of sample in the embodiment of the present invention one;
Fig. 3 is the X-ray powder diffraction figure of sample in the embodiment of the present invention one;
Fig. 4 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention two;
Fig. 5 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention three;
Fig. 6 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention four;
Fig. 7 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention five;
Fig. 8 is the magnetic hysteresis tropic comparison diagram of sample in the embodiment of the present invention one, four, five.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment one:
1-dimention nano chain Fe
3o
4the preparation method of/silk-protein mixture comprises the following steps:
(1) by 1.35g FeCl
36H
2o, 5.97g CH
3cOONa3H
2o joins in 60mL ethylene glycol solution, stirs until it dissolves completely;
(2) add the silk protein solution of 10mL mass percentage 7%, continue to be stirred to the homogeneous solution of formation;
(3) this mixed solution is poured in reactor, in 160 DEG C of reaction 36h, bottom reactor, place one block of Fe-Nd-B magnet simultaneously;
(4) reaction terminate after naturally cool to room temperature, and under the rotating speed of 8000rpm/min centrifuge washing (deionized water and ethanol respectively wash 3 times), finally by product in 60 DEG C of vacuum-dryings.
Fig. 1 and Fig. 2 is scanning electron microscope and the transmission electron microscope picture of sample, as can be seen from the figure, and Fe
3o
4nanoparticle and silk-protein mixture are spherical, and arrange chaining, and Fig. 3 is the X-ray powder diffraction figure of sample, show that the one-dimensional chain product synthesized is Fe
3o
4.
Embodiment two:
1-dimention nano chain Fe
3o
4the preparation method of/silk-protein mixture comprises the following steps:
(1) by 1.0g FeCl
36H
2o, 5.3g CH
3cOONa3H
2o joins in 50mL ethylene glycol solution, stirs until it dissolves completely;
(2) add the silk protein solution of 8mL mass percentage 7%, continue to be stirred to the homogeneous solution of formation;
(3) this mixed solution is poured in reactor, in 180 DEG C of reaction 24h, bottom reactor, place one block of Fe-Nd-B magnet simultaneously;
(4) reaction terminate after naturally cool to room temperature, and under the rotating speed of 8000rpm/min centrifuge washing (deionized water and ethanol respectively wash 3 times), finally by product in 60 DEG C of vacuum-dryings.
Fig. 4 is the scanning electron microscope (SEM) photograph of this sample, as can be seen from the figure, and Fe
3o
4nanoparticle and silk-protein mixture are spherical, and arrange chaining, and part has reunion.
Embodiment three:
1-dimention nano chain Fe
3o
4the preparation method of/silk-protein mixture comprises the following steps:
(1) by 1.5g FeCl
36H
2o, 5.0g CH
3cOONa3H
2o joins in 70mL ethylene glycol solution, stirs until it dissolves completely;
(2) add the silk protein solution of 12mL mass percentage 7%, continue to be stirred to the homogeneous solution of formation;
(3) this mixed solution is poured in reactor, in 200 DEG C of reaction 12h, bottom reactor, place one block of Fe-Nd-B magnet simultaneously;
(4) reaction terminate after naturally cool to room temperature, and under the rotating speed of 8000rpm/min centrifuge washing (deionized water and ethanol respectively wash 3 times), finally by product in 60 DEG C of vacuum-dryings.
Fig. 5 is the scanning electron microscope (SEM) photograph of this sample, as can be seen from the figure, and Fe
3o
4nanoparticle and silk-protein mixture are spherical, and arrange chaining.
Embodiment four:
Fe
3o
4the preparation of nanoparticle:
Its synthesis step is identical with embodiment one, only removes the step adding silk-protein.
Fig. 6 is the scanning electron microscope (SEM) photograph of this sample, can find out Fe
3o
4the pattern of nanoparticle is irregular, and it is serious to reunite, and can not present chain, show that the existence of silk-protein is the important factor of 1-dimention nano chain formation thus, is also form spherical Fe simultaneously
3o
4the important template of/silk-protein nano-complex.
Embodiment five:
Fe
3o
4the preparation of/silk-protein mixture:
Its synthesis step is identical with embodiment one, only removes the step of placing magnet bottom reactor.
Fig. 7 is the scanning electron microscope (SEM) photograph of this sample, can see, mixture is spherical, but it is serious to reunite, and can not be chain, show that externally-applied magnetic field is one of factor of 1-dimention nano chain formation thus.
Fig. 8 is the magnetic hysteresis tropic of three kinds of different samples, and in Fig. 8, a, b, c curve is respectively the magnetic hysteresis tropic of sample in embodiment one, embodiment four and embodiment five, as can be seen from the figure, and 1-dimention nano chain Fe
3o
4the saturation magnetic field of/silk-protein mixture is the highest, and not with the Fe of silk-protein
3o
4nanoparticle takes second place, and that minimum is the Fe not adding magnetic field
3o
4/ silk-protein mixture, illustrates in building-up process, and the magnetic of externally-applied magnetic field to mixture plays vital effect.
In sum, the present invention proposes one and prepare 1-dimention nano chain Fe
3o
4the method of/silk-protein mixture, the raw material sources of the method are extensive, and with low cost, synthesis technique is simple; Wherein, the template of employing is natural protein, silk-protein, and its Bc is good, environmental sound; In reaction, magnet is used to induce Fe as externally-applied magnetic field
3o
4the magnetic domain orientation of nanoparticle is consistent, makes mixture have stronger saturation magnetic field, enhances its performance, make its range of application wider.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (6)
1. a 1-dimention nano chain Fe
3o
4/ silk-protein mixture, is characterized in that: comprise Fe
3o
4nanoparticle and silk-protein, described Fe
3o
4nanoparticle is coated on described silk-protein and forms globular complex, and described in several, globular complex connects into chain.
2. 1-dimention nano chain Fe according to claim 1
3o
4the preparation method of/silk-protein mixture, is characterized in that: comprise the following steps:
(1) silk-protein and source of iron are dissolved in solvent, stir and disperse;
(2) solution in described step (1) is poured in reactor, bottom reactor, place one block of magnet, at 160-200 DEG C, react 1-36h;
(3), after having reacted, product is through washing, centrifugal and dry.
3. 1-dimention nano chain Fe according to claim 2
3o
4the preparation method of/silk-protein mixture, is characterized in that: described source of iron is FeCl
36H
2o, the mass percentage of described silk protein solution intermediate filment is 7%.
4. 1-dimention nano chain Fe according to claim 3
3o
4the preparation method of/silk-protein mixture, is characterized in that: described solvent is ethylene glycol, and described step (1) is first by CH
3cOONa3H
2after O and source of iron are dissolved in ethylene glycol, then add silk-protein, stir and disperse.
5. 1-dimention nano chain Fe according to claim 4
3o
4the preparation method of/silk-protein mixture, is characterized in that: described FeCl
36H
2o, CH
3cOONa3H
2the mass ratio of O, ethylene glycol and silk protein solution is: (1-1.5): (5-6): (55.5-77.7): (8-12).
6. 1-dimention nano chain Fe according to claim 2
3o
4the preparation method of/silk-protein mixture, is characterized in that: described magnet is Fe-Nd-B magnet.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510382554.7A CN104987731B (en) | 2015-07-03 | 2015-07-03 | 1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof |
| PCT/CN2015/089493 WO2017004893A1 (en) | 2015-07-03 | 2015-09-14 | One-dimensional fe3o4/fibroin composite nanochain and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510382554.7A CN104987731B (en) | 2015-07-03 | 2015-07-03 | 1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104987731A true CN104987731A (en) | 2015-10-21 |
| CN104987731B CN104987731B (en) | 2017-09-26 |
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|---|---|
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| WO (1) | WO2017004893A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801878A (en) * | 2016-04-11 | 2016-07-27 | 武汉纺织大学 | Preparation method of silk fibroin-based nano MOFs (metal-organic frameworks) |
| CN107552095A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | The silk three-dimensional porous material and preparation method of carried titanium dioxide Nano Silver |
| CN112537797A (en) * | 2020-12-07 | 2021-03-23 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN115998946A (en) * | 2022-12-15 | 2023-04-25 | 四川大学 | Magneto-electric response bionic oriented fiber hydrogel and preparation method and application thereof |
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| CN112980012A (en) * | 2021-02-22 | 2021-06-18 | 苏州大学 | Oriented material based on magnetic nanofiber and preparation method and application thereof |
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- 2015-09-14 WO PCT/CN2015/089493 patent/WO2017004893A1/en active Application Filing
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| CN101847479A (en) * | 2009-03-24 | 2010-09-29 | 中国科学院物理研究所 | Microwave composite material and preparation method thereof |
| CN103180364A (en) * | 2010-12-29 | 2013-06-26 | 韩华石油化学株式会社 | Biocompatible agent for dispersing nanoparticles into an aqueous medium using mussel adhesive protein-mimetic polymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105801878A (en) * | 2016-04-11 | 2016-07-27 | 武汉纺织大学 | Preparation method of silk fibroin-based nano MOFs (metal-organic frameworks) |
| CN107552095A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | The silk three-dimensional porous material and preparation method of carried titanium dioxide Nano Silver |
| CN112537797A (en) * | 2020-12-07 | 2021-03-23 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN112537797B (en) * | 2020-12-07 | 2023-04-18 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN115998946A (en) * | 2022-12-15 | 2023-04-25 | 四川大学 | Magneto-electric response bionic oriented fiber hydrogel and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN104987731B (en) | 2017-09-26 |
| WO2017004893A1 (en) | 2017-01-12 |
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